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Full text of "IS 5182 (Part 07): Methods for Measurement of Air Pollution, Part 07: Hydrogen Sulphide"

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IS 5182 (Part 07) (1973, Reaffirmed 2009) : Methods for 
Measurement of Air Pollution, Part 07: Hydrogen Sulphide. 
UDC 614.71 : 543.272.55 




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(Reaffirmed 2009) 



IS : 8182 (Fmt Vfl) - 1973 

( Reaffirmed 2003 ) 

Indian Standard 

METHODS FOR 
MEASUREMENT OF AIR POLLUTION 

PART VII HYDROGEN SULPHIDE 



Fourth Rcprinl JUNE 1995 
Oncotp&TZiittg AmeodnitDt No. J) 



UDC 614.71:543.272.55 



© Copyright 1982 

BUREAU OF INDIAN STANDARDS 

MANAK BHAVAN, 9 BAHADUR SHAH 2AFAII MARO 
NBW DRLHl 110003 

Gr 3 January 197< 



ISj5182( Part VD). 1973 

Indian Standard 

METHODS FOR 

MEASUREMENT OF AIR POLLUTION 

PART VII HYDROGEN SUiPHIDi 

Chemical Hazards Srctional Committee, CDC 18 

Chairman Rtpnstnim^ 

Brio G. R. Chait^ani Dirr^ctorateGrnrrai, Factory Advice Service 5t Labour 

Institutes. Bombay 

MembgfS 

SjiRi S. G, Kale { Aliernatt to 
Prig G. R. Chainani ) 
Shbi R. S. AoARWAr. Miniury of Drfence ( DGl ) 

Shri a. K. SiNnH ( Altirnale ) 
Shbx K. D. AmrB National Orsjanic Chemical Induftrir^ Lid, BomHay 

Shri J. P. Gkopka ( AlUsrnate) 
SflRi G. S. Apte Mmiitry i>r Feirolcum & Chemicals 

Shri K, Balastjbramaniam Kinc^ institute, M,idrai 

Shri K, R. Bur osu G<-ntral Public Hralth Kngincerini? Rwtarch Inilitute 

(CSIR), Naqpnr 
Snni B. N. Pathak {AiiernaU) 
Bnta P, R. Ckauhan National Safety Council, Bombay 

Chemist k MKTALi-TmoiflT-II, Railway Board ( Ministry ofRailwayi) 
Heskarch, Oraioifls awi> 
Stavdabds Orciamuation, 
LncKMOw 
Dr D. CitotrDHtiRY Indian Chemical Manufacturers' Asjociation, 

Calc\\tia 
Shri D. K. Sitik \r ( AlUrmfe) 
Shri j, M, D\\r, Mmisttv r>f Hralih & Family Planning (Department 

nfHrabh) 
Dr lArini^rt Shvntk^r Bhabha Aromic Research Centre, Bombay 

Shri JfvnmnKa Sinok Dir«morate General of Tcrhniral Development 

New Delhi 
Dr A, K. MiiKHKRTEfC Hindustan Steel Lid, Ranclii 

Si!RT O. V. SiNOH ( MUrnate) 
Slim M ? MvwHVMu Department of Rtplosivej { MmtUrv of Indunri.il 

Development ) 
Sjini K. Sans: ARAN ( AUemnU) 

{ Contmufff on pa^il) 



® Copyright 1982 
BUREAU OF INDIAN STANDARDS 

Tbis pubbcation la protected under the InSim Copyright Act (XIV of 1957) and 
rcproduciion in whole or in part by any mcflm except with written permission of 
the publisher shall be deemed to be an infrinfijemcnt of copyiight under the said Act. 



ISi$l«2(P«itVn)-1973 

( Cmiinuid/rom p^i \ ) 



SHU! O. P. Nakoia 



HindusUn Organic Chemic^U Ud, fUaaymui 
( Mahjirftfthtr») 
Su%t A« G. Sbbhak ( Aitm^) 
Shri N. D. Patwa wmam Minutry of Defence ( IXl! ) 

Sni%i R. M. Dteseit ( AltmMU) 
SAKt P. S. Ramacrahdiiah Difectorate General of Heftltli Servkei < Mini*8ry of 

Health & Family Planning ) 
Dfi S. S, CoTPHoaxAs ; ii/^ftnWii ) 
S«Rr D. Dah Gctta, Director Getiert^l, BIS ( Ex-i^tw Mmhtf ) 

Director ( Oiem) 

Smri a, K. Bhattaohahya 
Deputy Director ( Chem ), BIS 



Air Pollution Subcommittee, CDC 18:5 



Miniftlry ofHealth k Famiiy Plmninff { Departnvni 
ofHeahh) 



SkwJ. M, Dat« 

Sh»i R. S. Chatut Municipal Corporation of Greater Bombay 

Shri G. F. Khambatti ( AlttmaU ) 



DrG.C. Das 

Srri D. U. Hattikvptjh 

Shri N, V, Iykh 

Smri P. K. GotL ( AUtmats) 
Shri V. K. Ranaob 

Dr R, K. Dutta ( AUmaie ) 
Dr H. S. Rao 
Dr M.N.Rao 

Srri K. S. Somayaji 
Srri S. A. StrBRAicAi^xAN 

Dr D, G. Vyab 

SSKl P. K. Y«WKAWAR 

Sbri H. B. Sj^qb ( ^ii#7^/^ ) 



Calctiila Municipal Corpotaiion 

Cemeni Manufacturen' Asiociation. Bombay 

Indian Cmtitute of Peiroleum ( CSIR ). Dfhra Dun 

Hmdujtan Steel Led, Rancht 

Central Fuel Research Tmtituie ( CSIR), Dhanbad 
AU India Institute of Hygie?^e k Public Health, 

Calcutta 
Bhabha Atomic Research Centre, Bon^bay 
Central Water ft; Fovvcr Commiiiion ( Power Winff ), 

New Delhi ^ 

Ahtnedabed Municipal Corporttion 
C^enfral Publk Health Engmeetin^ Rtse&tch Imiitutt 

( CSIR ), Nagpuf 



I8i5182(Pfert Vn)-l»W 

Indian Standard 

METHODS FOR 
MEASUREMENT OF AIR POLLUTION 

PART VII HYDROGEN SULPHIDE 



a FOREWORD 

04 This Indian Standard (Part VII) was adopted by the Indian 
Standards Institution on 3 July 1973, after the draft finalised by the 
Chemical Hazards Sectional Committee had been approved by the 
Chemical Division Council. 

I>*2 Hydrogen sulphide is a highly toxic gas* Repeated exposure to low 
concentration has an irritating effect on mucous membranes, eyes and 
respiratory tract. 

®3 In reporting the result of a test or analysis made in accordance with 
this standard, if the Bnal value, observed or calculated, is to be rounded 
off, it shall be done in accordance with IS : 2-1960*. 



1. SCOPE 

LI This standard ( Part VII ) prescribes a method for the measurement 
of concentration of hydrogen sulphide in community air. 

Ll.l The range of concentration covered in this method is 6 p^gjrr? to 
600 /^g/m' of hydrogen sulphide in air. 

2- PIMNCIPLE 

2.1 The determination of hydrogen s^:iSphidt by color imcric method h 
based on the reaction which takes place under suitable conditions between 
Nj N-dimethyl-^-phcnylcncdlaminc sulphate, ferric sulphate and sulphide 
ions, resulting in the formation of methylene blue. 

♦Rules fof rounduig off numcrksl values ( nmgd)^ 

3 



IS J 5182 (Part VIIM973 
$. SENSmVITY 

3*1 Minimum detectable concentration of hydrogen sulphide is 0*03 ;ig 
per millilitre of the absorbing solution with an overall accuracy of ± 20 
percent. Beer's law is obeyed up to 2 ftg of hydrogen sulphide per milli'- 
litre of absorbing solution. 

4, INTERFERENCES 

4.1 Some strong rec(ucing agents like sulphites and thiosulphatcs prevent 
the formation of the colour or diminish its intensity. These may be 
climmated by adding sufficient awount of ferric sulphate solution. 

4*2 Atmospheric oxides of nitrogen cause interference. They may be 
avoided by adding sulphamic acid after the sampling is over. 

4.3 Other possible atmospheric interferences like sulphur dioxide, ozonc> 
and ammonia arc not serious at their normal existing levels ot 
concentrations. 

5. REAGENTS 

34 Absorbing Solirtloii — Dissolve 4'3 g of cadmium sulphate 
(CdS04 8HjO) in water. Add 0*3 g of sodium hydroxide dissolved in 
a small amount of water and dilute to one litre. Mix well before use, 
Store tiic soluiif>n in a refrl^ciatoi 

5.2 N^ N-Dlmethyl*^Pheayl€a^OiftmIiie*Sulphmte Solution — Add 

50 ml of concentrated sulphuiic acid ( conforming to IS : 266-1961*) to 
30 ml of distilled water and cool. Add 12 g of N, N-djmethyl-/?-i)henylenc 
diamine (H 2T2^ n{ N, N-dimethyl-^-phenylcne-diaminc sulphate. Stir 
the bulk solution nil it Is completely dissolved. Store Jt as stock solution 
m icfri^rerator 

5.2,1 For the purpose of prc])armg standards, dilute 25 ml of the stock 
solution to one litre with dilute sulphuric acid (1:1), 

S«} F«rric Sulphate Solutiosi — Add excess of ferric sulphate in 100 ml 
of water to ohK)m a sajMrafrd solutjrm. 

5.4 Siilphftmic Acid Solution ^ — 1 percent (m/y). Dissolve one grani 
of sulphamic acid m lOO ml of water. 

5.5 Sodium Sulpbide Solutiou — Dissolve 1*2 g of sodium sulphide ot 
analytical grade (Na^S. OH-.O), in one litre of pre-refrigerated distilled 
water and stopper it Since the solution is very unstable, it shall be pre- 
pared just before use. It shall be stored m a rcfiigcrator. Standardize 
this solution against standard sodium thiosulphatc solution ( 0*025 N) as 
follows. 



•Spectftcaiion for «u\phurK acid ( rtvu*d), 

4 



5.M Tak^ lOO ml of distilled water in 250-mt conic®! flask and add 
20 ml of standard iodine sokt8on(0-OT5 H ), Add 25 ml of hydrochloric 
acid (Oi N ) and fitraw with the tHiosulphate aolution usinf starch solu- 
tion M indicator. Note th« titmnt reading ai A, 

S.M Take 100 ml of distilled water in 25(%ml conical flask and add 
20 ml of standard iodine solution ( 0*025 N >. Add 25 ml of hydrochloric 
acid ( Oi N } and 20 ml of sodium sulphide soluiion ( 53) and repeat the 
titration with the thiosulphate solution. Note the tilrant reading ai B. 

3J3 Calculate the strength of sodium sulphide solution in terms of 
hydrogen sulphide as follows: 

^ufphfdr /ml « ^~^^ X normality of thiosulphate jtolution X i7x 10^ 

5«S*4 For the purpose of prcpariufr standards for comparison, dilute a 
portion of the sodium sulphide solution 50 that it contains equivalent of 
10 ^t?/ml of hydrogen sulphide. 

$. PREPARATION OF STANDARDS 

$A Prepare a set of different concentrations of hydrogen 5ulphide solution 
as follows, 

6.14 Arrange U tubes ( 50-ml capacity ) in line and put serial num* 
bers on them. 

6-1.2 Add 15 ml of absorbing solution to each tube. 

6.1.3 h^ indicated below, add to each of the 10 test-tubes an amount 
of dilute sodium sulphide solution necessary to give a concentration scries 
of 1 fi«f to 25 /Ag in increasing order: 

Tube No. Blank 123456789 10 

Amount in ml Oi 0*2 0'3 0*5 0*7 I'O 13 1*7 2-0 2-5 

of standard 
sulphide 
solution {>eg 
%SA ) 

6.1.4 Add 1 ml of suiphamic acid solution, 0*6 ml of N^N-dimethyU^- 
phcnylcnc-diamine sulphate solution ( S€$ 5*24 ), and 0*05 m! of ferric 
sulphate soJmion to each of the test-tubes in thai order, shaking well 
after each addition. 

64.5 Make up the volumes to 20 ml in each of the tubes with distilled 
water and mix thoroughly. 



ISi51t2(FanVn).I»73 

S.2 Pr@p@rsti0ffl of C!alit»nti<@ia Cmrv# 

S*24 Allow 30 minutea for the development of full colour in the tubes. 

6«2«2 Measure the colour intensity of the solutions in a spectrophoto« 
meter at 670 nm on transmission scale* Use the reagent blank as control. 

6.2.3 Draw the calibration curve of percent transmission vitsus micro- 
grams of hydrogen sulphide. 

7. SAMPLING APPARATUS 

74 The equipment to be used for sampling consists of a standard imptn- 
gcr of 35 ml capacity, a trap, a flowmeter or critical orifice device, and a 
suction pump. The arrangement of the sampling train is illustrated in 
Fig. 1. 








ml 
35 






30 













10 






5 


\l 


\ 



(MPINGER 



GLASS 
WOOL- 




TRAP 



Fio. 1 Sampling Train 
6 



ISj51tt(PartVII)-1973 

7.14 /m/jm^^fi — All-glass impingcr, 35 ml capacity, 220 mm in 
length ^nd 26 mm wide. Impinging end of the tube shall be of 1 mm 
bore size or preferably with fritted disc with porosity of 50 microns or 
less {s$0 Fig, 2A and2B). Impingers shall bt made from borosilicate 
glass. 



220 




130 



30 
10 



I 



^FRITT 



-^fOa? 00 
IMPINGINP, 

TUBE 



■a3tOa 26 00 
TUBE 



I 



♦ 



130 



M I 



^ 



30 



20 



15 



TED OfSC 

WITH POROSiry 

OF 50 MICRONS 
OR LESS 

lA PmiTED IMPI^GEH 




'410x7 00 
TUBE 



-23IDW600 



TUBE 



T" 

1mm RESTRlcnN& 
ORIFICE 



2B STANDARD IMPSNGEB 



AU dimcmiona in millimetres. 

Fjo. 2 Impinoer for Air Sampling 

7 



I8i5IS2 (PartVn)-I973 

74.2 FlowmUr — A rotameter calibrated accurately for the flow 
range from to 3 1/min, 

74.3 Cniical Orifia D^z/ia — This device is used to give a flow of 
about 1 I/min, Normally hypodennlc needles arc used as critical onficc. 
The needles shall be protected by mcmbianc filters. The arrangement is 
illustrated in Fig, '?. 




to 



ro 

Pump 




RUBBER 
SEPTUM 



HYPOOeRMiC 
NEFDLE 



MEMBRANE 
FtLfER 



Fro. 3 Critical Orifice Flow Device 



74.4 Trfl^— This may be a membrane filter [sa Fig. 3) ot a glass 
wool trap (^<*Fig. 2). 

74.5 Pump — It shall be a suction device, capable of drawing air 
into the sampling train at the rate of 10 to 20 I/min, provided with 
vacuum regulator and a moistuie trap. It shall be of light mass, suitable 
for field work (portable), with contmuous ratings self-lubzicating and 
capable of operating on 2i0 V ac, 50 Hz. 

i. PROCEDURE 

84 Sanpliisg 

844 Procedures arc described for short term { 30 minutes and 1 hour ) 
and for long term ( 24 hours ) sampling. One can select different combi- 
nations of sampling rate and time to meet special requirements. Sample 
volumes shall be adjusted, so that linearity is maintained between trans- 
mission and concentration over the dynamic range. 

^h2 Thirty- Minuie and One-Hour Samplings ~V'\2LCt 20 ml of 
the absorbinR solution in an impinger. Collect the sample at the rate of 
1 l/min for 30 minutes, or at 0'5 1/min for 1 hour using cither the 
rotameter, or a critical orifice device to control the fiow. Shield the 



absorbing rugent from direct sunlight during and after the sampling hy 
covcrin| the impinger with aluminium foil to prevent detenoratifta. 
Determine the volume of air sannpied by multiplying the flow rate by Ae 
time in minutes and record the atmospheric pressure and temperature. 
Remove and itoppcr the impinger. If the sample ia to be stored for more 
than a day before analysii, keep it at 5'G in a refrigerator* 

l«13 Twmiy Four-Hour Sampling — Place 20 ml of the absorbing 
solution in an impinger and collect the lample at the rate of 0'2 l/min for 
24 hours. Make sure that no entrainment of solution reauhs with the 
impinger. During collection and storage, protect from direct sunlight. 
Determine the total air volume by multiplying the air flow rate by the 
time in minutes. If storage is necessary, refrigerate the sample at 5*G. 

S.2 AsMlyais 

8.2^0 Gmsrol — Both the samples and each of the reagents to be used 
for analysis shall be dcoxygenatcd by passing & current of pure nitrogen 
through them for at least 5 minutes just before use. 

%1A SampU Prfparaiion -- U a precipitate is observed in the sample, 
rcnwjve it by ccntrifugation. 

••2.2 Add 1 ml of sulphamic acid solution. Add 0*6 ml of dilute 
N, N-dimcthyU/>-phcnylcnc diamine sulphate solution and 005 ml of ferric 
sulphate solution to the sample. Mix wdl by shaking the impinger after the 
additjon of each reagent. Make up the evaporation Josses by adding the 
absorbing solution to 20 ml mark of the impinger. Allow the mutturc to 
develop full colour by letting it stand for 30 minutes. Also prcpate 
a reagent blank following the above procedure* 

i.2.3 Measure the colour intensity ( percent transmission ) of the 
sample in a spectrophotometer at 670 nm. Compute from calibration 
curve the concentration in micrograms of hydrogen sulphide in the 
sample. 

f . CALCULATION 
t4 Hydrogen sulphide 

,*«/™%8 _^ micrograma o f hydrogen sulphide in the sample _ ,^ 

litres of air sampled 

No«B— 1 1^/Utfc hyarofea •ulpkide « QH ppm hydrofea »u!pia«k %i 25®C amd 
7fiO mmHf prewure. 



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